Method for preparing supported metallocene catalyst and supported metallocene catalyst prepared using the same
a technology of metallocene catalyst and catalyst, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, chemical/physical process, etc., can solve problems such as deterioration of catalytic activity
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preparation example 1
Preparation of First Metallocene Compound—[tBu—O—(CH2)6—C5H4]2ZrCl2
[0067]6-chlorohexanol was used to prepare tBu—O—(CH2)6—Cl according to the known method (Tetrahedron Lett. 2951 (1988)), and tBu—O—(CH2)6—Cl was reacted with NaCp to yield tBu—O—(CH2)6—C5H5 (yield: 60%; and b.p.: 80° C. / 0.1 mmHg). Zirconium (Zr) was attached in the same manner to yield tBu—O—(CH2)6—C5H4]2ZrCl2 (yield: 92%).
[0068]1H NMR (300 MHz, CDCl3): 6.28 (t, J=2.6 Hz, 2H), 6.19 (t, J=2.6 Hz, 2H), 3.31 (t, 6.6 Hz, 2H), 2.62 (t, J=8 Hz), 1.7-1.3 (m, 8H), 1.17 (s, 9H);
[0069]13C NMR (CDCl3): 135.09, 116.66, 112.28, 72.42, 61.52, 30.66, 30.61, 30.14, 29.18, 27.58, 26.00.
preparation example 2
Preparation of Second Metallocene Compound—tBu—O—(CH2)6)(CH3)Si(C5(CH3)4)(tBu—N)TiCl2
[0070]At the room temperature, to a 10 L reactor were added 50 g of Mg(s) and then 300 ml of THF. About 0.5 g of I2 was added to the reactor, which was then kept at 50° C. Once the reactor temperature gets stable, 250 g of 6-t-buthoxyhexyl chloride was added to the reactor at a rate of 5 ml / min through a feeding pump. With the addition of 6-t-buthoxyhexyl chloride, the reactor temperature was increased by about 4 to 5° C. The reactor was stirred for 12 hours while 6-t-buthoxyhexyl chloride was continuously added. The 12-hour reaction resulted in a black solution. 2 ml of the black solution was collected and mixed with water to form an organic layer, which was then subjected to 1H-NMR to identify 6-t-buthoxyhexane. The analysis of the 6-t-buthoxyhexane showed that the Grignard reaction took place actively, thereby synthesizing 6-t-buthoxyhexyl magnesium chloride.
[0071]500 g of MeSiCl3 and 1 L of THF...
example 1
Preparation of Supported Metallocene Catalyst
[0076]Carrier
[0077]Silica (XPO2410 manufactured by Grace Davison) was used as a carrier.
[0078]Immobilization of MAO
[0079]To a glass reactor were added 10 g of the silica as a carrier, 100 ml of toluene, and then a methylaluminoxane (MAO) solution containing 40 mmol of aluminum in toluene. The resultant solution was stirred at 80° C. for one hour to bring about a gradual reaction. Then, the MAO solution containing 40 mmol of aluminum was added again to the reactor, which was under agitation at 50° C. for one hour to initiate a gradual reaction. The resultant solution was washed with an excess of toluene to eliminate the aluminum compound remaining without participating in the reaction.
Preparation of Supported Metallocene Catalyst
[0080]To the MAO-immobilized catalyst was added a toluene solution containing a second metallocene compound. The resultant solution was stirred at 40° C. for one hour to initiate the reaction. After addition of a t...
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